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. 2023 Aug 24;13(36):25459–25463. doi: 10.1039/d3ra04608g

Optimisation of reaction conditions ab.

graphic file with name d3ra04608g-u1.jpg
Entry Change from conditions above 3a (%)
1 None 54%
2 Addition of 5 eq. pyridine 55%
3 Addition of 5 eq. 2,6-lutidine 53%
4 30 mol% 1 55%
5 20 mol% TEMPO in place of 1 52%
6 No 1 added 25%
7 10 mA c
8 No current 0%
9 0.1 M [TBA][PF6] in place of LiClO4 20%
10 0.1 M [TBA][BF4] in place of LiClO4 13%
11 0.1 M [TBA][ClO4] in place of LiClO4 21%
12 0.1 M NaClO4 in place of LiClO4 42%
13 0.5 mmol 2a and reaction time of 3 h 43%
14 0.5 mmol 2a and reaction time of 6 h 98%
15 2 mmol 2a and reaction time of 24 h 99%
16 0.5 mmol 2a, 3h, Pt anode, Ni cathode 46%
17 0.5 mmol 2a, 3h, glassy carbon anode, Ni cathode 41%
18 0.5 mmol 2a, 3h, graphite anode, Pt cathode 35%
a

Reactions performed on the 1 mmol scale unless stated otherwise.

b

Product conversion determined by 1H-NMR spectroscopy.

c

Significant electrode fouling observed.